CN104775041A - Clean vanadium extraction method for self-circulation utilization of vanadium-solution-calcium-process precipitated vanadium, mother liquor and solid waste - Google Patents
Clean vanadium extraction method for self-circulation utilization of vanadium-solution-calcium-process precipitated vanadium, mother liquor and solid waste Download PDFInfo
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Abstract
The invention provides a clean vanadium extraction method for self-circulation utilization of vanadium-solution-calcium-process precipitated vanadium, mother liquor and solid waste, which comprises the following steps: adding a calcification additive into a purified vanadium solution to perform calcium-process vanadium precipitation reaction, carrying out immersion reaction on the obtained calcium vanadate, and crystallizing the obtained ammonium vanadate solution to obtain an ammonium metavanadate crystal. The vanadium solution calcification vanadium precipitation-carbonating immersion-crystal separation method is adopted to implement regeneration and cyclic utilization of the vanadium extraction additive sodium salt. The Na and V in the vanadium solution are separated to thoroughly implement zero discharge and medium utilization on the vanadium precipitation wastewater. The conventional vanadium precipitation technique of removing vanadium, chromium and ammonia from wastewater and other terminal treatment processes are removed, and the chromium in the wastewater is recovered in the product and sold at high value. The solid waste except vanadium extraction tailings in the technique is circularly utilized in the process, and the vanadium extraction tailings enter an iron and steel process so as to be recycled.
Description
Technical field
The invention belongs to vanadium field of chemical metallurgical technology, relate to the clean extraction vanadium method that the precipitation of a kind of vanadium liquid calcium method, mother liquor and solid waste self-circulation utilize, particularly relate to a kind of containing the chemical industry extraction vanadium method of vanadium material sodium vanadium extraction-calcium method precipitation-mother liquor with " solid waste " recycle.
Background technology
The traditional method that Vanadium Pentoxide in FLAKES is produced is vanadium slag sodium roasting-ammonium salt precipitation method, and wherein the vanadium product of more than 65% comes from this method.The ammonium salt precipitator method have two kinds: a kind of is first the pH value of the solution containing pentavalent vanadium is adjusted to 8.5 ~ 9.5, then presses V in solution
2o
5ammonium salt Precipitation ammonium meta-vanadate is added with mass ratio 1:1.3 ~ 1.5 of ammonium salt; Another kind adopts substep to reconcile pH value to 1.5 ~ 2.5 of solution, adds ammonium salt Precipitation ammonium poly-vanadate, after the ammonium meta-vanadate obtained or ammonium poly-vanadate are obtained Vanadium Pentoxide in FLAKES through calcining.
The main deficiency of this technique is: (1) Vanadium in Vanadium Residue mainly exists with vanadium iron spinel structure, and chemical mine is stablized mutually, is difficult to decompose; In gas-solid calcination process, oxygen mass transfer weak effect, even if adopt multiple high temp roasting, the recovery per pass of vanadium also only has 80%; This technique cannot avoid this deficiency.(2) contain more siliceous low melting point in vanadium slag, improving temperature of reaction will cause ring formation, affect the operation of kiln, limit the further raising of temperature of reaction, and the method be therefore difficult to by improving temperature improves the extraction yield of vanadium.(3) the ammonium process of sinking can produce a large amount of high salinity, nitrogen-containing wastewater, and unit vanadium product (in Vanadium Pentoxide in FLAKES) waste water generation is about 40 tons, serious environment pollution; Ton vanadium chrome waste water treatment cost is at about 3000 yuan, and improvement cost is large.
CN 101157478A proposes a kind of preparation method of ammonium poly-vanadate, with traditional sodium roasting-water logging explained hereafter containing vanadium solution for raw material, vanadium is first made to generate calcium vanadate with the calcium chloride added or nitrocalcite, then turn molten with bicarbonate of ammonia, vanadium enters solution, calcium generates the calcium carbonate of more indissoluble, the vanadium liquid sulphur acid for adjusting pH after separation, and precipitation obtains ammonium poly-vanadate.This technique, compared with traditional technology, the alkali content in ammonium poly-vanadate can be dropped to less than 0.1%, and in vanadium wastewater, ammonia content is down to 60% ~ 75% of traditional technology, but is there is the emission problem of ammonia nitrogen waste water.
In view of existing vanadium slag sodium roasting-water logging vanadium extraction, stone coal sodium roasting vanadium-extracting utilize technical progress to be difficult to meet the strategic requirement of vanadium cleaner Production in Chemical Industry, therefore must research and develop the method realizing vanadium high efficiente callback vanadium liquid from source, exploitation solves the vanadium liquid vanadium extraction clearer production technology of environmental pollution.
Summary of the invention
For the problem of prior art, an object of the present invention is to provide a kind of high-efficiency cleaning extraction vanadium method, further object of the present invention is the clean extraction vanadium method providing the precipitation of a kind of vanadium liquid calcium method, mother liquor and solid waste self-circulation to utilize, described method wastewater zero discharge, technical process is short, easy and simple to handle, production cost is low.
To achieve these goals, present invention employs following technical scheme:
The clean extraction vanadium method that the precipitation of vanadium liquid calcium method, mother liquor and solid waste self-circulation utilize, comprises the following steps:
After purification, vanadium liquid adds calcification additive and carries out calcium method precipitation reaction, then the calcium vanadate that obtain is occurred to turn leaching reaction, the Ammonium Vanadate Solution crystallization obtained is obtained ammonium meta-vanadate crystal.
Preferably, said method comprising the steps of:
(1) to purification after vanadium liquid add calcification additive, carry out in atmospheric conditions the precipitation of calcium method reaction, be separated obtain calcium vanadate precipitation and NaOH solution;
(2) the calcium vanadate ammonium bicarbonate soln that step (1) obtains is sized mixing, carry out turning leaching reaction, be separated and obtain Ammonium Vanadate Solution and precipitation of calcium carbonate;
(3) Ammonium Vanadate Solution crystallisation by cooling step (2) obtained or add ammonium salt crystallization, is separated and obtains ammonium meta-vanadate crystal and crystalline mother solution;
Optionally, step (4) is carried out:
(4) decomposed through high-temperature calcination by the calcium carbonate that step (2) obtains, regeneration obtains CaO, and it can be used as calcification additive, prepare calcium vanadate for step (1), calcium source is able to recycle.
The present invention adopts vanadium liquid calcium precipitation-carbonating to turn the method for molten-Crystallization Separation, can realize regeneration and the recycle of additive for extracting vanadium sodium salt.
Preferably, described calcification additive is CaO and/or Ca (OH)
2.
In the present invention, described separation can be filtering separation.
The treating processes of vanadium probably comprises: roasting, leaching, purification and precipitation, the present invention be namely by purification after vanadium liquid carry out above-mentioned technique.In the present invention, preferably adopt containing the vanadium extraction of vanadium material sodium roasting technique, then leach, purification.
Therefore, preferably, after purification vanadium liquid be vanadium slag or bone coal etc. containing after vanadium minerals raw material sodium roasting water logging vanadium extraction containing vanadium solution.
Preferably, described calcification additive addition is 1.5 ~ 3 to add according to Ca/V mol ratio, and now in vanadium liquid, the deposition rate of vanadium is higher than 95%, and the V element content in calcium vanadate is 20 ~ 26wt%.Described molar ratio is as being 1.6,1.7,1.8,1.9,2.0,2.1,2.2,2.3,2.4,2.5,2.6,2.7,2.8 or 2.9.
Preferably, described calcium method precipitation temperature of reaction is 40 ~ 100 DEG C, now in vanadium liquid the deposition rate of vanadium higher than 95%, such as 45 DEG C, 50 DEG C, 55 DEG C, 60 DEG C, 65 DEG C, 70 DEG C, 75 DEG C, 80 DEG C, 85 DEG C, 90 DEG C or 95 DEG C, reaction times is 10 ~ 50min, such as 15min, 20min, 25min, 30min, 35min, 40min or 45min.
Preferably, during NaOH concentration < 150g/L in step (1) vanadium liquid, the NaOH solution that step (1) obtains directly returns leaching and the washing procedure of " vanadium bearing slag ", the precipitation of the Leaching Vanadium liquid repeating step (1) obtained and lock out operation.In above process, the NaOH medium of the 8 ~ 50wt% leaching and obtain after washing procedure is stayed and is soaked in vanadium tailing soil, and when re-baking, (with Naization additive form) is directly utilized.50 ~ 92wt% (namely remaining) NaOH medium is stayed in Leaching Vanadium liquid, the precipitation of repeating step (1) and lock out operation, and the NaOH concentration after making each circulating leaching in vanadium liquid gets a promotion.
Preferably, when after the NaOH concentration enrichment in step (1) vanadium liquid to >=150g/L, for ensureing calcium method precipitation effect, NaOH solution evaporation concentration step (1) obtained is that the NaOH solution of 40 ~ 80wt%, 40 ~ 80wt% returns as sodium additive and all utilizes containing vanadium minerals burden process to NaOH concentration.Preferably, when the NaOH solution that step (1) obtains is containing chromium, chromium will in evaporative process crystallization, obtain Sodium chromate product after refining.
Preferably, described turn of leaching temperature of reaction is 20 ~ 100 DEG C, such as 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C or 90 DEG C, turning the leaching reaction times is 10 ~ 100min, such as 20min, 30min, 40min, 50min, 60min, 70min, 80min or 90min, turning leaching reaction liquid-solid ratio is 4:1 ~ 10:1, such as 5:1,6:1,7:1,8:1 or 9:1.
Preferably, the ammonium bicarbonate soln concentration in step (2) is 1 ~ 40wt%, such as 5wt%, 10wt%, 15wt%, 20wt%, 25wt%, 30wt% or 35wt%.
Preferably, the crystallisation by cooling terminal temperature in step (3) is 0 ~ 50 DEG C, such as 5 DEG C, 10 DEG C, 15 DEG C, 20 DEG C, 25 DEG C, 30 DEG C, 35 DEG C, 40 DEG C or 45 DEG C.
Preferably, step (3) adds ammonium salt to ammonium salt concentration is 5 ~ 50wt%, such as 10wt%, 15wt%, 20wt%, 25wt%, 30wt%, 35wt%, 40wt% or 45wt%.
Preferably, the calcium vanadate that the crystalline mother solution that step (3) obtains returns for step (2) turns leaching.
Preferably, step (4) described calcining temperature is 900 ~ 1000 DEG C.
Compared with the prior art, the present invention has following beneficial effect:
1. additive for extracting vanadium sodium salt is regenerated and recycle; 2. be separated by Na, V in vanadium liquid, the zero release and the mediumization that thoroughly realize precipitation " waste water " utilize; 3. eliminate the end treatment processes such as conventional precipitation processing wastewater " three take off " (vanadium removal, de-chromium, deamination), the chromium in waste water is sold by commercialization recovery, high level; 4. except tailings in vanadium extraction, technique " solid waste " utilizes at flow process internal recycle, and tailings in vanadium extraction enters iron and steel process resourcesization and utilizes.5. present invention achieves efficient vanadium extracting, vanadium yield reaches more than 98%.Therefore, present method is the method for clean and effective vanadium extraction.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Technical scheme of the present invention is further illustrated by embodiment below in conjunction with accompanying drawing.
Embodiment 1: the clean extraction vanadium method processing step that the precipitation of this vanadium liquid calcium method, mother liquor and solid waste self-circulation utilize is as described below:
(1) calcification precipitation: add milk of lime in Leaching of Vanadium from Vanadium slag liquid after purification, addition is 1.5 times of V molar weight in liquid phase, precipitation temperature is 40 DEG C, reaction 100min, obtain calcium vanadate and NaOH concentration is the alkaline solution of 150g/L, it is 40% that alkaline solution is evaporated to NaOH concentration, obtains crystals of sodium chromate and crystalline mother solution, crystalline mother solution is used for vanadium slag sodium roasting additives, and crystals of sodium chromate purity after refining is 99.0%;
(2) bicarbonate of ammonia turns molten: it is molten that calcium vanadate adds ammonium bicarbonate soln transfer, obtain Ammonium Vanadate Solution and calcium carbonate, wherein ammonium bicarbonate soln concentration is 1%, turns that a molten process reaction temperature is 20 DEG C, the reaction times is 10min, and turning a molten process liquid-solid ratio is 10:1;
(3) Crystallization Separation vanadium: Ammonium Vanadate Solution is cooled to 10 DEG C of crystallizations, obtains ammonium meta-vanadate crystal and crystalline mother solution, mother liquor returns calcium vanadate and turns molten operation;
(4) calcium source regeneration: calcium carbonate obtains CaO after 900 DEG C of calcinings, returns calcification precipitation operation.
After testing, calculate, in the present embodiment, vanadium comprehensive yield is 98.5%.
Embodiment 2: the clean extraction vanadium method processing step that the precipitation of this vanadium liquid calcium method, mother liquor and solid waste self-circulation utilize is as described below:
(1) calcification precipitation: add milk of lime in extracting vanadium from stone coal liquid after purification, addition is 3.0 times of V molar weight in liquid phase, and precipitation temperature is 100 DEG C, reaction 10min, obtain calcium vanadate and NaOH concentration is the alkaline solution of 10g/L, alkaline solution returns bone coal grog and leaches operation;
(2) bicarbonate of ammonia turns molten: it is molten that calcium vanadate adds ammonium bicarbonate soln transfer, obtain Ammonium Vanadate Solution and calcium carbonate, wherein ammonium bicarbonate soln concentration is 10%, turns that a molten process reaction temperature is 100 DEG C, the reaction times is 10min, and turning a molten process liquid-solid ratio is 4:1;
(3) Crystallization Separation vanadium: it is 50% that Ammonium Vanadate Solution supplements bicarbonate of ammonia to concentration, obtains ammonium meta-vanadate crystal and crystalline mother solution, mother liquor returns calcium vanadate and turns molten operation;
(4) calcium source regeneration: calcium carbonate obtains CaO after 1000 DEG C of calcinings, returns calcification precipitation operation.
After testing, calculate, in the present embodiment, vanadium comprehensive yield is 98.3%.
Embodiment 3: the clean extraction vanadium method processing step that the precipitation of this vanadium liquid calcium method, mother liquor and solid waste self-circulation utilize is as described below:
(1) calcification precipitation: add unslaked lime in Leaching of Vanadium from Vanadium slag liquid after purification, addition is 2.0 times of V molar weight in liquid phase, and precipitation temperature is 50 DEG C, reaction 50min, obtain calcium vanadate and NaOH concentration is the alkaline solution of 35g/L, alkaline solution returns vanadium slag grog and leaches operation;
(2) bicarbonate of ammonia turns molten: it is molten that calcium vanadate adds ammonium bicarbonate soln transfer, obtain Ammonium Vanadate Solution and calcium carbonate, wherein ammonium bicarbonate soln concentration is 30%, turns that a molten process reaction temperature is 50 DEG C, the reaction times is 20min, and turning a molten process liquid-solid ratio is 5:1;
(3) Crystallization Separation vanadium: it is 40% that Ammonium Vanadate Solution supplements bicarbonate of ammonia to concentration, obtains ammonium meta-vanadate crystal and crystalline mother solution, mother liquor returns calcium vanadate and turns molten operation;
(4) calcium source regeneration: calcium carbonate obtains CaO after 1000 DEG C of calcinings, returns calcification precipitation operation.
After testing, calculate, in the present embodiment, vanadium comprehensive yield is 98.8%.
Embodiment 4: the clean extraction vanadium method processing step that the precipitation of this vanadium liquid calcium method, mother liquor and solid waste self-circulation utilize is as described below:
(1) calcification precipitation: add unslaked lime to not purifying in Leaching of Vanadium from Vanadium slag liquid, addition is 2.5 times of V molar weight in liquid phase, and precipitation temperature is 80 DEG C, and reaction 50min, obtains calcium vanadate and NaOH concentration is the alkaline solution of 100g/L;
(2) bicarbonate of ammonia turns molten: it is molten that calcium vanadate adds ammonium bicarbonate soln transfer, obtain Ammonium Vanadate Solution and calcium carbonate, wherein ammonium bicarbonate soln concentration is 40%, turns that a molten process reaction temperature is 80 DEG C, the reaction times is 15min, and turning a molten process liquid-solid ratio is 6:1;
(3) Crystallization Separation vanadium: Ammonium Vanadate Solution is cooled to 50 DEG C of crystallizations, obtains ammonium meta-vanadate crystal and crystalline mother solution, mother liquor returns calcium vanadate and turns molten operation;
(4) calcium source regeneration: calcium carbonate obtains CaO after 950 DEG C of calcinings, returns calcification precipitation operation.
After testing, calculate, in the present embodiment, vanadium comprehensive yield is 98.9%.
Applicant states, the present invention illustrates method detailed of the present invention by above-described embodiment, but the present invention is not limited to above-mentioned method detailed, does not namely mean that the present invention must rely on above-mentioned method detailed and could implement.Person of ordinary skill in the field should understand, any improvement in the present invention, to equivalence replacement and the interpolation of ancillary component, the concrete way choice etc. of each raw material of product of the present invention, all drops within protection scope of the present invention and open scope.
Claims (10)
1. the clean extraction vanadium method that vanadium liquid calcium method precipitation, mother liquor and solid waste self-circulation utilize, comprises the following steps:
After purification, vanadium liquid adds calcification additive and carries out calcium method precipitation reaction, then the calcium vanadate that obtain is occurred to turn leaching reaction, the Ammonium Vanadate Solution crystallization obtained is obtained ammonium meta-vanadate crystal.
2. the method for claim 1, is characterized in that, said method comprising the steps of:
(1) to purification after vanadium liquid add calcification additive, carry out in atmospheric conditions the precipitation of calcium method reaction, be separated obtain calcium vanadate precipitation and NaOH solution;
(2) the calcium vanadate ammonium bicarbonate soln that step (1) obtains is sized mixing, carry out turning leaching reaction, be separated and obtain Ammonium Vanadate Solution and precipitation of calcium carbonate;
(3) Ammonium Vanadate Solution crystallisation by cooling step (2) obtained or add ammonium salt crystallization, is separated and obtains ammonium meta-vanadate crystal and crystalline mother solution;
Optionally, step (4) is carried out:
(4) decomposed through high-temperature calcination by the calcium carbonate that step (2) obtains, regeneration obtains CaO, and it can be used as calcification additive, prepare calcium vanadate for step (1), calcium source is able to recycle.
3. method as claimed in claim 1 or 2, it is characterized in that, described calcification additive is CaO and/or Ca (OH)
2;
Preferably, after purification vanadium liquid be containing after vanadium minerals raw material sodium roasting water logging vanadium extraction containing vanadium solution.
4. the method as described in one of claim 1-3, is characterized in that, described calcification additive addition is 1.5 ~ 3 interpolations according to Ca/V mol ratio;
Preferably, described calcium method precipitation temperature of reaction is 40 ~ 100 DEG C, and the reaction times is 10 ~ 50min.
5. the method as described in one of claim 2-4, it is characterized in that, during NaOH concentration < 150g/L in step (1) vanadium liquid, the NaOH solution that step (1) obtains directly returns leaching and the washing procedure of " vanadium bearing slag ", the precipitation of the Leaching Vanadium liquid repeating step (1) obtained and lock out operation;
Preferably, the NaOH medium of the 8 ~ 50wt% leached and obtain after washing procedure is stayed and is soaked in vanadium tailing soil, directly utilized when re-baking, the NaOH medium of 50 ~ 92wt% is stayed in Leaching Vanadium liquid, the precipitation of repeating step (1) and lock out operation.
6. the method as described in one of claim 2-5, it is characterized in that, when after the NaOH concentration enrichment in step (1) vanadium liquid to >=150g/L, NaOH solution evaporation concentration step (1) obtained is that the NaOH solution of 40 ~ 80wt%, 40 ~ 80wt% returns as sodium additive and all utilizes containing vanadium minerals burden process to NaOH concentration;
Preferably, when the NaOH solution that step (1) obtains is containing chromium, chromium will in evaporative process crystallization, obtain Sodium chromate product after refining.
7. the method as described in one of claim 1-6, is characterized in that, described turn of leaching temperature of reaction is 20 ~ 100 DEG C, and turning the leaching reaction times is 10 ~ 100min, and turning leaching reaction liquid-solid ratio is 4:1 ~ 10:1.
8. the method as described in one of claim 2-7, is characterized in that, the ammonium bicarbonate soln concentration in step (2) is 1 ~ 40wt%.
9. the method as described in one of claim 2-8, is characterized in that, the crystallisation by cooling terminal temperature in step (3) is 0 ~ 50 DEG C;
Preferably, step (3) adds ammonium salt to ammonium salt concentration is 5 ~ 50wt%;
Preferably, the calcium vanadate that the crystalline mother solution that step (3) obtains returns for step (2) turns leaching.
10. the method as described in one of claim 2-9, is characterized in that, step (4) described calcining temperature is 900 ~ 1000 DEG C.
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| CN107522218A (en) * | 2017-10-19 | 2017-12-29 | 河钢股份有限公司承德分公司 | A kind of ultrasound-enhanced calcium vanadate ammonium leaching and the method for preparing nano-calcium carbonate |
| CN107746078A (en) * | 2017-11-28 | 2018-03-02 | 河钢股份有限公司承德分公司 | A kind of system and method for preparing ammonium metavanadate crystal |
| CN107964601A (en) * | 2017-11-24 | 2018-04-27 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method of chromium content in reduction calcium vanadate |
| TWI635184B (en) * | 2017-06-05 | 2018-09-11 | 虹京金屬股份有限公司 | Method for recovery of vanadium in vanadium-containing waste catalyst |
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| CN109402401A (en) * | 2018-12-11 | 2019-03-01 | 中国科学院过程工程研究所 | A kind of method of high calcium cleaning vanadium extraction containing vanadium raw materials |
| CN110668497A (en) * | 2019-11-01 | 2020-01-10 | 河钢股份有限公司承德分公司 | Method for preparing vanadium and chromium products from vanadium-chromium-containing double salt and application of vanadium and chromium-containing double salt |
| CN110835696A (en) * | 2019-11-26 | 2020-02-25 | 河钢股份有限公司承德分公司 | Preparation method of vanadium pentoxide |
| CN111748702A (en) * | 2020-07-06 | 2020-10-09 | 攀钢集团研究院有限公司 | Method for preparing vanadium oxide and circulating sodium and ammonium by using vanadium solution |
| CN113979474A (en) * | 2021-11-26 | 2022-01-28 | 中国科学院过程工程研究所 | Method for internal circulation of ammonium carbonate medium in process of preparing vanadium pentoxide from calcium vanadate |
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| TWI635184B (en) * | 2017-06-05 | 2018-09-11 | 虹京金屬股份有限公司 | Method for recovery of vanadium in vanadium-containing waste catalyst |
| CN107522218A (en) * | 2017-10-19 | 2017-12-29 | 河钢股份有限公司承德分公司 | A kind of ultrasound-enhanced calcium vanadate ammonium leaching and the method for preparing nano-calcium carbonate |
| CN107964601A (en) * | 2017-11-24 | 2018-04-27 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method of chromium content in reduction calcium vanadate |
| CN107964601B (en) * | 2017-11-24 | 2019-06-14 | 攀钢集团攀枝花钢铁研究院有限公司 | A kind of method of chromium content in reduction calcium vanadate |
| CN107746078A (en) * | 2017-11-28 | 2018-03-02 | 河钢股份有限公司承德分公司 | A kind of system and method for preparing ammonium metavanadate crystal |
| CN107746078B (en) * | 2017-11-28 | 2023-08-11 | 河钢股份有限公司承德分公司 | System and method for preparing ammonium metavanadate crystals |
| CN108754125A (en) * | 2018-08-21 | 2018-11-06 | 中南大学 | A kind of vanadium-containing material sodium roasting vanadium-extracting cleaning procedure |
| CN108754125B (en) * | 2018-08-21 | 2020-08-04 | 王懿 | Clean process for extracting vanadium from vanadium-containing material through sodium salt roasting |
| CN109402401B (en) * | 2018-12-11 | 2020-12-04 | 中国科学院过程工程研究所 | Method for cleanly extracting vanadium from high-calcium vanadium-containing raw material |
| CN109402401A (en) * | 2018-12-11 | 2019-03-01 | 中国科学院过程工程研究所 | A kind of method of high calcium cleaning vanadium extraction containing vanadium raw materials |
| CN110668497A (en) * | 2019-11-01 | 2020-01-10 | 河钢股份有限公司承德分公司 | Method for preparing vanadium and chromium products from vanadium-chromium-containing double salt and application of vanadium and chromium-containing double salt |
| CN110835696A (en) * | 2019-11-26 | 2020-02-25 | 河钢股份有限公司承德分公司 | Preparation method of vanadium pentoxide |
| CN111748702B (en) * | 2020-07-06 | 2022-05-24 | 攀钢集团研究院有限公司 | Method for preparing vanadium oxide and circulating sodium and ammonium by using vanadium solution |
| CN111748702A (en) * | 2020-07-06 | 2020-10-09 | 攀钢集团研究院有限公司 | Method for preparing vanadium oxide and circulating sodium and ammonium by using vanadium solution |
| CN114574699A (en) * | 2020-12-01 | 2022-06-03 | 中国科学院过程工程研究所 | Method for preparing ammonium metavanadate and ammonium molybdate from vanadium-molybdenum-containing solution |
| CN114574699B (en) * | 2020-12-01 | 2024-03-12 | 中国科学院过程工程研究所 | Method for preparing ammonium metavanadate and ammonium molybdate from vanadium-molybdenum-containing solution |
| CN113979474A (en) * | 2021-11-26 | 2022-01-28 | 中国科学院过程工程研究所 | Method for internal circulation of ammonium carbonate medium in process of preparing vanadium pentoxide from calcium vanadate |
| CN115259223A (en) * | 2022-07-27 | 2022-11-01 | 中国科学院过程工程研究所 | Method for preparing ammonium metavanadate by using calcium vanadate |
| CN115259223B (en) * | 2022-07-27 | 2023-11-14 | 中国科学院过程工程研究所 | Method for preparing ammonium metavanadate from calcium vanadate |
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